Presence of Helium (⁴₂He, ³₂He) Confirmed in Deuterated Pd-black
by the "V_i Effect" in a "closed QMS" Environment

By Yoshiaki ARATA & Yue-Chang ZHANG

Proceedings of the Japan Academy, April, 1997
Communicated April 14, 1997

Although helium is generally quite insoluble in metals, large amounts of this element can be stored within a highly deuterated host metal such as Pd-black as a result of deuterium nuclear reactions continuously generated over long periods. However, since it is almost impossible for these helium atoms to then escape from the Pd-black host to the surrounding environment at ambient temperatures, to confirm their presence it is absolutely essential that Pd-black samples be heated to high temperatures to expel whatever helium they may contain. Therefore, to confirm the existence of helium atoms generated from deuterium in samples of Pd-black, we simply employed the "sample heating" process (room temperature1500º C), but carried it out using both a "QMS" system and a super-high vacuum "Getter pump" inside a totally sealed vessel. We termed this methodology "closed QMS", and developed a related discrimination method which applies an opportunely changing voltage to the anticipated elements present inside the "closed QMS" environment (including helium). Measurements were then taken as the applied voltage was both increased and decreased between 7020[V] (the range being determined by the ionizing voltage V_i[V] for helium series elements). Using this principle, which we call the "V_i effect", we were able to conclusively confirm the presence of both ⁴₂He and ³₂He atoms, as well as their relative ratio. It is evident that development of both the "closed QMS" system and the "V_i effect" methodology were vital to finally prove the presence of helium generated by deuterium nuclear fusion within highly deuterated Pd-black.

Keywords : Helium (⁴₂He, ³₂He); cold fusion; Pd-black; closed QMS; "V_i-effect"

To prove the existence of a deuterium nuclear reaction inside a solid, the following five key processes proved necessary. (In other words, only after comprehending and applying the principles or methodologies outlined in the five steps below was it possible to achieve "cold fusion" and conclusively confirm its empirical reality.

1) First key: Creation of an intensely pressurized, highly deuterated host metal (even more concentrated than solid body density).

A Double Structure cathode ("DS cathode") had to be fabricated using Pd-black as the inner cathode enclosed within a vacuum sealed "Pd vessel" which functions as the outer cathode.

• Note 1) : The "Pd vessel" rapidly supplies pure D⁺ ions to the Pd-black during electrolysis via the "spillover effect" and extremely high interior D₂ gas pressure (several thousand [atm]) in accordance with Sievertz' well known law. That is to say, both the phenomena respectively described by the "spillover effect" and "Sievertz law" are indispensable to the function of the "DS cathode.

• Note 2) : Pd-black (dia400 Å) rapidly absorbs D+ ions at almost 100% efficiency due to intrinsic physical phenomena such as "atom clustering".

The authors noted the impenetrable resistance metal generally presents to the passage of helium, effectively preventing either its entry or escape. This led to the conclusion that if a nuclear fusion reaction were to occur within a metal, in this case Pd-black, a large amount of helium would perforce be held fast and retained inside.

3) Third key : Recognition of the special prerequisites for releasing helium from metal

Helium can only escape from a metal when the latter is heated to high temperature and/or dissolved in a liquid solution. The former method is far superior for accurately and reliably detecting helium, because helium atoms can be released simply by using the standard "Sample Heating" process (room temperature 1500º (C).

The authors developed a "closed QMS" (Quadrupole Mass Spectrometer) system which has thus far proven indispensable for identifying and measuring helium at high levels of accuracy and reliability.

• Note 1): Samples are placed inside the "closed QMS" environment at ultra-high vacuum and for long periods ( 3x10^-9 Torr, 10 hrs).
• Note 2) : The conditions outlined in Note 1 assure that the QMS only detects elements/compounds released from the "Heated Sample" itself and is minimally disturbed by ambient contaminants.
• Note 3) : Inside the "closed QMS" system, the effect of "Getter action" (at least to its practical limits) eventually eliminates or radically diminishes all adulterating constituents (here, the hydrogen series elements/compounds) leaving only the helium series elements.

The authors developed a new discrimination method based on the "V_i effect" (authors' term) which distinguishes helium in a "closed QMS" environment in terms of its known ionizing voltage (V_i [volt]). Using this method, the existence of both ⁴₂He and ³₂He was not only positively established, the ⁴₂He/³₂He ratio was also accurately ascertained.

When a diversity of elements exist inside a closed vessel, they can be separated and classified into discrete groups (A, B, C, D...) in terms of their ionizing voltages (V_i [volt]). That is, group A will be defined by the same V_i (A), group B by identical V_i (B), etc.

For example, when V_i (A) = 13.5 [V] and V_i (B) = 24.5 [V], group A corresponds to the hydrogen series and group B to the helium series as follows:

Group A: hydrogen series ( (H, D, T), (H₂, D₂, T₂), (DH, TH, DT), (D₂H, DH₂, TH₂, T₂H, TD₂, T₂D), (H₃, D₃, T₃)
Group B : helium series (⁴₂He, ³₂He)

In conditions where these two groups exist together we may consider the combination itself as an inclusive group and define it as:

Group C : an intermixture of groups A and B.

In the situation above, each of the elements or molecules belonging to these groups can be further classified in terms of its mass M_n (n=1, 2, 3...n). For example, when n=2, n=3, n=4 (i.e., the necessary mass numbers for detecting the presence of hydrogen and helium):
Group A : n=2 (M₂: H₂, D), n=3 (M₃: DH, T, H₃), n=4 (M₄: D₂, TH)
Group B : n=2 (M₂: ---), n=3 (M₃: ³₂He), n=4 (M₄: ⁴₂He)
Group C : n=2 (M₂: H₂, D), n=3 (M₃: ³₂He, DH, T, H₃), n=4 (M₄: ⁴₂He, D₂, TH)

In general, when no significant amounts of tritium (and/or its compounds) exist in a given environment, it is clear that "H₂"> > D, "DH" > > T, and "D₂" > > TH. In which case, it is reasonable to conclude that preponderantly M₂="H₂", M₃="DH"+ ³₂He, and M₄="D₂"+ ⁴₂He.

If we want to know whether or not helium exists among the substances within a closed vessel, it must therefore be demonstrated whether elements with mass M₂ and M₃ whose V_i =24.5 [V] are present inside it.

It is well established that when an applied voltage (V_app) on an element group is lower than its ionizing voltage (V_i), it cannot be detected by QMS. For instance, if V_app ( 24.0 [eV], then group A elements (V_i = 13.5 [V]) can be clearly detected, but group B elements (V_i = 24.5 [V]) cannot be detected at all. This made it possible to separate and clearly distinguish groups A and B as represented in curves "A" and "B" in Fig. 1. Using this "V_i effect", as we have termed the principle, within a "closed QMS" environment, we then demonstrated the characteristics of group C (including both A and B groups) and logically plotted it as curve "C" in Fig. 1 below.

a) Logical "V_i-effect" curve.The existence of helium among the diverse elements released from non-deuterated Pd-black or highly deuterated Pd-black can be conclusively confirmed by employing the "V_i effect" within a "closed QMS" environment. If helium exists in a "closed QMS" environment, we can logically deduce the "V_i effect" curve as shown in Figure 2.

Confirmation of helium's presence just requires testing for mass numbers M₂, M₃ and M₄ as only these cover both the hydrogen and helium series. In view of the "V_i effect", the intensity and normalized curves for each of these may be logically plotted as illustrated in Figure 2 graphs (A), (B) and (C) respectively.

Thus the hydrogen series can be seen to concentrate entirely in normalized curve "A" whereas the helium series is indicated solely by normalized curve "B". Therefore, non-deuterated samples which contain no helium should demonstrate only curve "A", while highly deuterated samples should be distinguished by curve "C" (under normal conditions with "A" and B*), but will generate both curves "A" and "B" or simply curve "B" alone if no "DH" or hydrogen series elements/compounds are available.

b) Actual experimental "V_i-effect" curves for some Pd-black samples. Fig. 3 shows experimental "V_i-effect" data for non-deuterated samples demonstrating the absence of the helium series. The logical "V_i-effect" curves shown in Fig. 2 and Fig. 4 . Fig. 5 display experimental data for highly deuterated samples clearly demonstrating the presence of helium (³₂He, ⁴₂He and the ³₂He/⁴₂He ratio.) These data all coincide with the logical "V_i-effect" curve in Fig.2.

Although the ³₂He/⁴₂He ratio ( [He*]) was found to be [He*] 4 in a previous report¹, the results of this experiment incorporating many runs and samples showed [He*] to be distributed across a range 2~10.

Figure 1

Fig. 1 : Experimental "V_i effect" curves for non-deuterated Pd-black = Graphs (A ) & (C), and highly deuterated Pd-black = Graphs (B ) & (D).

NOTE: Using a non-deuterated sample, the forms of both curves M₂ ("H₂") and M₃ ("DH") in Graph (A) entirely coincide as the superimposition in Graph (C) illustrates. However, in a highly deuterated sample as shown in Graph (B), the hydrogen region ( V_app the form of the M₃ curve coincides with the M₂, just as in Graph (C), while in the helium region (Vapp25 [V]) visibly diverge (shadowed area) as shown in Graph (D). This separated zone quantitively correlates with the presence of ³₂H. In this case, a ratio of [He*] (⁴₂He/³₂He) 4 was obtained, but over the course of many samplings, ratios ranging from [He*] 2~10 were also encountered as noted herein.

Figure 2

Fig. 2 Logical characteristics of the "V_i effect" curve for elements released from non-deuterated Pd-black ([D*]=0) and highly deuterated Pd-black ([D*]1).

• Note 1) : Whether using no sample whatever or using only non-deuterated Pd-black, when measured in a "closed QMS" environment, the intensities for both conditions should essentially demonstrate the hydrogen series curves (M₂: "H₂", M₃: "DH", M₄: "D₂") in graph (A) and the normalized curve "A" shown in graph (B).
• Note 2) : Graph (C) shows normalized data for a composite mixture including both hydrogen-series and helium-series elements/compounds. Normalized curves "A", "B" and "C" ("C" ="DH" + ³₂He, "C₀"="D₂" + ⁴₂He* ) respectively illustrate the logical characteristics of the hydrogen series, the helium series, and their admixture. These are thus the characteristics that a highly deuterated Pd-black sample must exhibit to demonstrate the presence of helium. Because "D₂" is easily diminished by "Getter action", curve "C₀" is generally not evident because it homologizes to "B" ("C₀"=⁴₂He="B") and usually only curve "C" remains.
• Note 3) : Because even "DH" is greatly abated by "non-evaporative Getter action", "C" also tends to homologize to "B" ("C" = ³₂He="B", just as "C₀"=⁴₂He="B"). Therefore, the logical "V_i effect" curves for elements released from highly deuterated Pd-black in a "closed QMS" environment should finally only show curve "A" for "H₂" and curve "B" signifying the helium series (⁴₂He, ³₂He) as shown in graph (B).

Graph (A)

• Note 1) : Logical intensity curves corresponding to the "V_i effect" for each element of group A (hydrogen series : "H₂", "DH", "D₂") and group B (helium series: ⁴₂He, ³₂He )
• Note 2) : Non-deuterated Pd-black signifies group A only.
• Note 3) : Highly deuterated Pd-black indicates both A and B groups: (M₂= "H₂"), (M₃= "DH" + ³₂He) and (M₄="D₂"+ ⁴₂He).

Graph (B)

• Note 1) : Logical normalized "V_i effect" curves "A" and "B" for each of the intensity curves for groups A and B in graph (A).
• Note 2) : Non-deuterated Pd-black signifies group A only.
• Note 3) : Highly deuterated Pd-black will indicate both A and B groups when "D₂" and "DH" disappear inside the "closed QMS" environment as explained in the next note for graph (C).

• Note 1) : Logical normalized "V_i effect" curves for "C" ("C" and "C₀") for group C including both A and B groups.
• Note 2) : Although highly deuterated Pd-black is usually represented by graph (C), when normal "Getter action" is applied in a "closed QMS" environment, "D₂" finally disappears and curve "C₀" homologizes to curve "B" ("C₀"=⁴₂He="B") leaving only curve "C". Moreover, the use of still stronger "Getter action" eliminates even "DH" and thus also homologizes curve "C" to "B" ("C"=³₂He="B"). The logical normalized curves thus reduce to only "A" and "B" as shown in graph (B).

Graph (D)

• Note 1) : When curve "C" signifies M₃ (=³₂He + "DH") and "extended C" forms the same curve as the hydrogen series (curve "A"), then the ratio ³₂He/"DH" = b/a.

Figure 3

Fig. 3 Characteristics of the V_i-effect" curve for non-deuterated Pd-black ([D*]=0).

• Note 1) : Data (a₀) and (b₀) respectively correspond to the intensity curves for the hydrogen series and normalized curve "A" in Fig. 2.
• Note 2) : M₄ ("D₂") could not be detected because it was greatly abated by "Getter action".
• Note 3) : Curves of the "B" and "C" type (as shown in Fig. 2) do not appear at all, demonstrating that no helium series elements whatever exist in this sample.

Figure 4

Fig. 4 Characteristics of the V_i-effect" curve for highly deuterated Pd-black ([D*]1).

• Note: This data shows remarkable correspondence to Graphs (A) and (C) in Fig. 2, and decisively demonstrates the existence of helium (⁴₂He, ³₂He), in this case with a ⁴₂He/³₂He ratio 3

.

Figure 5

Fig. 5 : "V_i-effect" curve for some samples of highly deuterated Pd-black.

• Note : The ratios of ⁴₂He/³₂He ([He*]) show some range of distribution. For instance, [He*] = 3, 10, 4, 10, and 4 for Data (a₁, b₁), (a₂, b₂), (a₃, b₃), (a₄, b₄), and (a₅, b₅), respectively.

This study was conducted through a research grant from the Japan Academy. The authors would like to thank Prof. Y. Imai, M.J.A., and Prof. T. Nagamiya, M.J.A., for their intellectual support for this study; Prof. Emeritus K. Sugimoto of Osaka and Tokyo Universities and Prof. Emeritus H. Fujita of Osaka University for their comments; ULVAC Japan, Ltd, Mr. K.Yanagishita, and CRIEPI's Dr. Y. Asaoka for their assistance; and the staff members of JWRI, Osaka University, and President F. Kawakami of Sulzer Meteco, Jpn, Ltd, for their encouragement.

Reference

1. Arata, Y. and Zhang, Y.C. (1996) Proc. Japan Acad. 72B, 179-184, and 73b, 1-6.

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